反应详情

To a stirred solution of (0.048 g, 0.575 mmol) 2-amino-oxazole [Cockerill & al., Synthesis 591(1976)], and DMAP (0.003 g, 0.03 mmol) in pyridine (2 ml) was added at 0° C. (0.100 g, 0.384 mmol) 9H-thioxanthene-9-carbonyl chloride. Stirring was continued at RT for 16 h, the reaction mixture was evaporated and water (5 ml)/sat. NaHCO3 solution (2 ml) was added. The solid was filtered off, dissolved in dichloromethane, dried (MgSO4), and concentrated in vaccuo. The crude material was purified by column chromatobraphy on silica gel (methylene chloride/ methanol 40:1) to give the product (0.022 g, 18%) as a white solid, m.p. 188-191° C. and MS: m/e=309.1 (M+H+).

1. customthe reaction mixture was evaporated
2. additionNaHCO3 solution (2 ml) was added
3. filtrationThe solid was filtered off
4. dissolutiondissolved in dichloromethane
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vaccuo
7. customThe crude material was purified by column chromatobraphy on silica gel (methylene chloride/ methanol 40:1)